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A kind of preparation method of ultra-thin high oxygen permeability dual-phase dense oxygen-permeable film and its prepared product

A technology of high oxygen permeability and oxygen permeable membrane, applied in the direction of separation method, semi-permeable membrane separation, chemical instruments and methods, etc., can solve the problems of reduced mechanical strength, increased difficulty of testing and packaging, etc., and achieves low production cost, good chemical Compatibility, effect of improving oxygen permeability

Inactive Publication Date: 2019-07-16
JINGDEZHEN CERAMIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the diaphragm is thinned to a certain extent, it will bring a series of problems such as reduced mechanical strength and increased difficulty in testing and packaging, which cannot meet the requirements of practical applications.

Method used

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  • A kind of preparation method of ultra-thin high oxygen permeability dual-phase dense oxygen-permeable film and its prepared product
  • A kind of preparation method of ultra-thin high oxygen permeability dual-phase dense oxygen-permeable film and its prepared product
  • A kind of preparation method of ultra-thin high oxygen permeability dual-phase dense oxygen-permeable film and its prepared product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In this embodiment, a method for preparing an ultra-thin high-oxygen-permeability dual-phase oxygen-permeable membrane, the steps are as follows:

[0033] (1) Preparation of porous SDC matrix layer

[0034] (1-1) According to the stoichiometric ratio, Ce(NO 3 ) 3 ·6H 2 O, Sm(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, and according to the volume ratio SDC:template Ni(NO 3 ) 2 ·6H 2 O=6:4 adding template Ni(NO 3 ) 2 ·6H 2 O, using cetyltrimethylammonium bromide (CTAB) as a surfactant and NaOH as a precipitating agent, wherein according to the molar ratio of metal ions: CTAB: NaOH = 1: 1.5: 2, SDC was prepared by coprecipitation and Ni(OH) 2 Mix the precursors, and then calcinate in an air atmosphere at 800°C for 2h to obtain a mixture powder of SDC and NiO;

[0035] (1-2) The above-mentioned SDC and NiO mixture powder was dry-pressed at 120MPa, calcined in air at 1400°C for 6h, and then in pure H 2 Treat at 800°C for 4h in the atmosphere, reduce NiO to...

Embodiment 2

[0040] In this embodiment, a method for preparing an ultra-thin high-oxygen-permeability dual-phase oxygen-permeable membrane, the steps are as follows:

[0041] (1) Preparation of porous SDC matrix layer

[0042] According to the volume ratio SDC powder (commercial): graphite particles = 6: 4, ball milling and mixing to obtain a uniform SDC and graphite mixture, after 120MPa dry pressing, calcining at 800°C for 2h in air to obtain a porous SDC matrix layer;

[0043] (2) Preparation of dual-phase film layer

[0044] (2-1) Preparation of CCO powder: Ca(NO 3 ) 2 , Co(NO 3 ) 2 Dissolve in deionized water, add citric acid and EDTA according to the molar ratio of metal ion:citric acid:EDTA=1:1.5:1, stir for 2h, and continue stirring in a water bath at 80°C until the water evaporates to form a gel, and then Heated on a furnace until it burns to form Ca 3 co 2 o 6 Precursor powder; the Ca 3 co 2 o 6 Grind the precursor powder, put it into an electric furnace for roasting, ...

Embodiment 3

[0047] In this embodiment, a method for preparing an ultra-thin high-oxygen-permeability dual-phase oxygen-permeable membrane, the steps are as follows:

[0048] (1) Preparation of porous SDC matrix layer

[0049] (1-1) According to the stoichiometric ratio, Ce(NO 3 ) 3 ·6H 2 O, Sm(NO 3 ) 3 ·6H 2 O was dissolved in deionized water, and according to the volume ratio SDC:template Ni(NO 3 ) 2 ·6H 2 O=6:4 adding template Ni(NO 3 ) 2 ·6H 2 O, using cetyltrimethylammonium bromide (CTAB) as a surfactant and NaOH as a precipitating agent, wherein according to the molar ratio of metal ions: CTAB: NaOH = 1: 1.5: 2, SDC was prepared by coprecipitation and Ni(OH) 2 Mix the precursors, and then calcinate in an air atmosphere at 800°C for 2h to obtain a mixture powder of SDC and NiO;

[0050] (1-2) The above-mentioned SDC and NiO mixture powder was dry-pressed at 120MPa, calcined in air at 1450°C for 6h, and then in pure H 2 Treat at 800°C for 4h in the atmosphere, reduce NiO ...

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Abstract

The invention discloses a preparation method of an ultrathin biphase dense oxygen-permeation membrane with a high oxygen transmission rate and a product prepared by the preparation method. The preparation method comprises the following steps: firstly, preparing a porous SDC matrix layer by a self-sacrificing template method; secondly, coating a low-oxygen partial pressure end with a complex of an ion conductive phase SDC and an electronic conductive phase CCO by a silk-screen printing method or a vacuum spin coating method; thirdly, carrying out cofiring to form a layer of ultrathin dense SDC-CCO biphase membrane layer on the surface of the SDC matrix layer, thus obtaining an asymmetric biphase dense oxygen-permeation membrane. Besides, the invention also discloses a product prepared by using the preparation method. According to the preparation method disclosed by the invention, an ultrathin dense SDC-CCO biphase membrane layer can be obtained on the surface of the porous SDC matrix layer, so a transmission path of oxygen ions is greatly shortened; meanwhile, the strength of a membrane is effectively ensured, and the packaging of the membrane is facilitated; the preparation method can be widely applied to the fields of oxygen separation in air, partial oxidation of methane, oxygen-enriched combustion and the like.

Description

technical field [0001] The invention relates to the technical field of functional ceramic materials, in particular to a method for preparing an ultra-thin, high-oxygen-permeability dual-phase dense oxygen-permeable membrane and a product thereof. Background technique [0002] The mixed conductor dense membrane has a very high oxygen permeability at high temperature, and can be used as a gas separation membrane to separate and produce oxygen from oxygen-containing gases. It is suitable for the preparation of pure oxygen and the partial oxidation of methane to synthesis gas (CO / H 2 ), methane oxidative coupling to hydrocarbons, oxygen-enriched combustion and other processes have attracted great attention and research in the past ten years. [0003] According to the phase composition of the material, the mixed conductor membrane can be divided into a single-phase oxygen-permeable membrane and a two-phase oxygen-permeable membrane. For single-phase oxygen permeable membranes, m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01D67/00B01D53/22
CPCB01D53/228B01D67/0039B01D71/024B01D2325/24
Inventor 谢志翔陈婷江伟辉李月明
Owner JINGDEZHEN CERAMIC UNIV